Process of manufacturing nitroglycerin.



.FRANZ XIGNER, OF POTSDAM, ERMANY, A

GESELLSGHAFT VORMALS ALFRED NOBEL UNI) 00., or HAMBURG, GERMANY.

I To all whom *it may concern:

ject of the Emperor of Au: Mia-Hungary, re

'r onsicn SSIGNOILTO THE FIRM OF DYNAMIT-ACTIEN- rnocnssor MANUFACTURING NITRO LYCERIN.

Be it known tnatl, FRANZ AIG LR, a 'su briding at 10 Neue Konigdra-zse, Potsdam, Kingdom of Prussia, German Empire, li. ave invented new and useful Improvements in. Processes of Manufacturing Nitroglycerin, of which the following is a specification.

This invention relates to the proccss of inan'ufactuirng nitro-glycerin by causing a mixture of nitricacid and sulfuric acid to act on glycerinfand has for its object to render the process more expeditious, considerably safer and cheaper.-.

The common nitro-glycerin di rs from the'usual process of manufacturing nitro -cellulose among other things essentially in that the waste acids from the nitration of glycerin cannot be revived but must be denitrated'. The reason of the said difference that-tho nitrating acids of the nitroglycerin-lmanufacture are used up by thenltratmg process .111 a lar' er degree than'in the manufacture of nitrocel u-v lose." From these reasons the waste acids of the nitro-glygcerin :manufacture', that have been separated from the nitro-glycerin bysettling etc .iare with referen'ceto theirjconiposition by far inferiorto those of the nitro cellulose manufacture.

I have now found that the reviving of the wasteacids of the nitro-glycerin manufacture (which acids contain glycerin oom P ds)- the composition v vnitr grams pure ultra-glycerin in nitrating 100 gives an unexpected advantage, because I'BVlVGd waste acid gives an essent ally higher .arnount of nitroglycerin than the original nitrating acid 'with the same relative proportions of sulfuric acid, nitric acid and Water in the same manner of operation. The reviving of the waste acid containing glycerin compounds is effected by adding a fresh mixture of highly concentrated sulfuric and nitric acid to thewaste acid in a suitable proportion.

In nitrating 100 grams of glycerin witl 900 grams of freshly prepared nitrating acid of for instance obtained 2Olfgra1hs pure g ycerin. I obtained,. .however, 228

grams glycerin with. 900 grams-of a once ffprocess of manufacturing PatentedFeb. 23, 1909.

' revived nitrating acid of'tZ-e same relative proportions of acids and water 1 (H 30, :HNQ, 11 0.; :30:10),

but composed of 450 grains of waste acidfrom a previous nitrating operation and 450 grams fresh acid; A similar favorable result was obtained by a furt'..cr use of the already .once revived nitrating acid containing glycerin compounds: I obtained 225 grams pure nltro-glycerinby nitrating 100 grams gly'c prim with 900 grams nitrating acid, twice re vlved, of tLe same relative proportions of acids and water quoted I (I1 SO IlIiNO -II'I O 60 :30 :10)

ing acid is used. .I obtained 170 grains pure.

nitro-glycerin by nitrating 100 grains glyc erin with 1200 grams fresh nitrating acid of the compositlon 11 0- 1.11:IIIIII idea? I obtained however 218 grams pure nitroglycerin, l. e. surplus of. 48 grams over the quoted amount, by nitrating 100 grams glycerin with 1200 grams once' revived nitrating acidof the same relative proportions of acids and water as quoted v (H SO zHNO zH O 56722832150) but composed of 7 50 grams waste acid from the first nitration and 450 grams fresh nitrating acid. A twice revived waste acid of the same percentage gave 221 grams pure Intro-glycerin, 'i. e. a surplus of 51 grams when compared with the result of the fresh nitrating acid; One can obtain the said advantage, of an increased yield of pure ntro-glycerin by using revived nitrating acid even with acids containing 20 per cent. water, 'i. e. approaching to those acid mixtures which cannot have any nitrating action. 1

The difference in the nitrating action 110 by using fresh out the forn'iation of froth by tain from 1.1 to

between a revived nitrating acid and a fresh acid has been quite unknown in the manul facture oi." nitro-cellulose. The possibility by using revived acids of obtaining essentially higher amounts of nitro-glycerin than acids enables the operator to var the degree of concentration of nitrating aci s in a relatively wide range and espe less concentrated nitrating l acids, the use of which was formerly uneconomical in the prior process without re- The concentration of .the usual for manufacturing nitro-glyc i only by 5 per cent. 1t? has been considered hitherto by all experts as'near'ly unavoidable to use only acids of the highest concentration in order to prevent a reduction of the yield of nitroglycerin to below 200 grains ol pure nitroglycerin, the average yield being 205 grams pure intro-glycerin from 100 grams glycerin. 3y the possibility given by the present invention of using acids with '10 and even 15 per cent. water one obtains the further advantage of a greater security for the nitrating operation. For instance I obtain. an essentially gentle nitration of glycerin withusing a nitrateially to use viving. nitratmg acid erin dlflered hitherto ing acid of the composition (H SOJ-INO JI O=60:30:1O)

according to my method instead of the usual mixture.

11,30 60% use n 0 5% lhe greater yield of t1'initroglycerin ohtained by using the waste. acid instead of l fresh acids alone is not caused by nitro-l glycerin suspended. in the spent acid. By l causing wast e acid from nit-rating, glycerin to stand for a suilirivnt time, one can only oh- 1.4% trinitroglyr-erin. By l a far greater l the present process, however The common slightly soluble in acids and separates thereyield of trinitroglyeerin can be, obtained than by causing the waste acid to stand. The inventor has also stated the reason for the increasing of the 'ield of trinitroglycerin by using a waste acid. In the nitrating )rocess carried out in the ordinary way, esides trinitroglycerin (i. e. the common nitroglycerin) relatively large amounts of lower nitrated nitroglycerins (dinitro lycerin and monoglycerin) will be genera ly formed. trinitroglycerin now is very fore quickly and relatively completely. 'T he mononitroglyeerin and dinitrogl cerin are, however, very soluble in acids and can there fore not separate, even by very long standing. Mononitroglycerin and dinitroglyeerin are converted into trinitroglycerin, it one causes fresh nitrating acids to act on them. ()nthis the new process is based.

What 1 claim as my invention, to secure by Letters Patent, is-

The proc ss of nitrating glycerin to obtain a maximum yield of trinitro-glycerin from successively treated portions of glycerin, which consists in nitrating a quantity of glycerin with a suitable quantity of a and desire fresh mixture of concentrated nitric and sulfuric acids, separating the resultant trinitro-glycerin from the partially exhausted acids, containing less highly nitrated .derivatiyes of glycerin, adding a suitable quantity of fresh concentrated nitric and sulfuric acids to restore the acid mixture to sub stantially its original percentage content of nitric acid, sulfuric acid and water, and

" nitrating' a second portion of glycerin with said acid mixture, substantially as described. In testimony whereof I have signed my name to this specification in the presence of two subscribing witnesses.

FRANZ AlllNlCll. \Vitncsses:

Wow mun l'imr'r, ll cam llASlER. 

